Métodos de produção eficientes que economizam tempo e energia são sempre exigidos e novos processos de sinterização de baixo custo têm sido desenvolvidos para materiais cerâmicos e implementados por empresas e pesquisadores em todo o mundo. Com este objetivo, uma nova abordagem conhecida como Flash Sintering está atraindo grande interesse. Esta nova técnica de sinterização envolve a aplicação de campo elétrico através de uma amostra durante o aquecimento, gerando assim aceleração abrupta da cinética de densificação, diminuindo o tempo de sinterização de horas para segundos e diminuindo o aquecimento do forno em até centenas de graus Celsius. Frequentemente descritas para cerâmicas policristalinas e compósitos de cerâmica e vidro, a sinterização auxiliada por campo elétrico com apenas vidro não foi encontrado na literatura. A sinterização assistida por campo elétrico foi controlada com sucesso, sem que ocorresse o escoamento da amostra, obtendo uma elevada densidade relativa do vidro comercial. Um vidro de janela soda-cal-sílica não estequiométrica foi usado na pesquisa devido à sua importância comercial, por ser um material de partida de baixo custo, por apresentar condução iônica e haver na literatura dados de propriedades físicas e de cinética de sinterização convencional. O campo elétrico também influencia fortemente a cinética de sinterização do vidro soda-cal-sílica. Os resultados experimentais foram comparados com cálculos analíticos realizados a partir do modelo de Clusters não-isotérmico de sinterização de vidro por fluxo viscoso com cristalização concorrente. O aumento de temperatura nos compactos de pó de vidro durante o aquecimento do forno e aplicação de campo elétrico foi estimado usando um modelo de radiação de corpo negro. Preliminarmente, o aumento da temperatura devido ao efeito Joule pode explicar a diminuição da temperatura de amolecimento em comparação com a temperatura do forno e a sinterização rápida do vidro estudado. / Efficient production methods saving time and energy are always demanded and novel reduced-cost sintering processes have being developed for ceramic materials and implemented by companies and researchers of all over the world. With this aim, a new sintering approach generally known as flash sintering is attracting great interest. This new sintering technique involves the application of electric field through a sample while heating, thereby generating abrupt acceleration of the densification kinetics, decreasing the sintering time from hours to seconds and decreasing the oven heating in up to hundreds of degrees Celsius. Well described for polycrystalline ceramics and ceramic-and-glass composites, the sintering of pure glass aided by electric field is still lacking in the literature. The sintering assisted by electric field, was successfully controlled, without sample flow, achieved a high relative density of a commercial glass. A non-stoichiometric soda-lime-silica window glass was used due to its commercial importance, low cost starting material, ionic conduction, and literature on physical properties and conventional sintering kinetics. Electric field was observed to also strongly influence window glass sintering kinetics. The experimental results were compared with analytical calculations obtained from the non-isothermal Clusters model of glass sintering by viscous flow with concurrent crystallization. The temperature increase in the glass powder compacts during oven heating and electric field application was estimated by using a black-body radiation model. Preliminary, the temperature increase due to Joule effect can explain the softening temperature decrease compared with the oven temperature, and the fast sintering of the studied glass.

Métodos de produção eficientes que economizam tempo e energia são sempre exigidos e novos processos de sinterização de baixo custo têm sido desenvolvidos para materiais cerâmicos e implementados por empresas e pesquisadores em todo o mundo. Com este objetivo, uma nova abordagem conhecida como Flash Sintering está atraindo grande interesse. Esta nova técnica de sinterização envolve a aplicação de campo elétrico através de uma amostra durante o aquecimento, gerando assim aceleração abrupta da cinética de densificação, diminuindo o tempo de sinterização de horas para segundos e diminuindo o aquecimento do forno em até centenas de graus Celsius. Frequentemente descritas para cerâmicas policristalinas e compósitos de cerâmica e vidro, a sinterização auxiliada por campo elétrico com apenas vidro não foi encontrado na literatura. A sinterização assistida por campo elétrico foi controlada com sucesso, sem que ocorresse o escoamento da amostra, obtendo uma elevada densidade relativa do vidro comercial. Um vidro de janela soda-cal-sílica não estequiométrica foi usado na pesquisa devido à sua importância comercial, por ser um material de partida de baixo custo, por apresentar condução iônica e haver na literatura dados de propriedades físicas e de cinética de sinterização convencional. O campo elétrico também influencia fortemente a cinética de sinterização do vidro soda-cal-sílica. Os resultados experimentais foram comparados com cálculos analíticos realizados a partir do modelo de Clusters não-isotérmico de sinterização de vidro por fluxo viscoso com cristalização concorrente. O aumento de temperatura nos compactos de pó de vidro durante o aquecimento do forno e aplicação de campo elétrico foi estimado usando um modelo de radiação de corpo negro. Preliminarmente, o aumento da temperatura devido ao efeito Joule pode explicar a diminuição da temperatura de amolecimento em comparação com a temperatura do forno e a sinterização rápida do vidro estudado. / Efficient production methods saving time and energy are always demanded and novel reduced-cost sintering processes have being developed for ceramic materials and implemented by companies and researchers of all over the world. With this aim, a new sintering approach generally known as flash sintering is attracting great interest. This new sintering technique involves the application of electric field through a sample while heating, thereby generating abrupt acceleration of the densification kinetics, decreasing the sintering time from hours to seconds and decreasing the oven heating in up to hundreds of degrees Celsius. Well described for polycrystalline ceramics and ceramic-and-glass composites, the sintering of pure glass aided by electric field is still lacking in the literature. The sintering assisted by electric field, was successfully controlled, without sample flow, achieved a high relative density of a commercial glass. A non-stoichiometric soda-lime-silica window glass was used due to its commercial importance, low cost starting material, ionic conduction, and literature on physical properties and conventional sintering kinetics. Electric field was observed to also strongly influence window glass sintering kinetics. The experimental results were compared with analytical calculations obtained from the non-isothermal Clusters model of glass sintering by viscous flow with concurrent crystallization. The temperature increase in the glass powder compacts during oven heating and electric field application was estimated by using a black-body radiation model. Preliminary, the temperature increase due to Joule effect can explain the softening temperature decrease compared with the oven temperature, and the fast sintering of the studied glass.

Ce travail porte sur l'évolution microstructurale d'un alliage TiAl lors du frittage par un procédé appelé Spark Plasma Sintering (SPS). Les poudres initiales, élaborées par atomisation, sont constituées principalement d'une phase métastable. Les transformations qui accompagnent le retour à l'équilibre de cette dernière durant un chauffage sont finement caractérisées par MEB, MET et EBSD. Ces transformations seront ensuite utilisées comme marqueur thermique lors de la densification SPS afin de mieux estimer les amplitudes des gradients thermiques et mécaniques du procédé de frittage. Les mécanismes de densification responsables de la formation des cous sont discutés, ainsi que les origines des hétérogénéités microstructurales des échantillons complètement densifiés. Un comparatif des mécanismes de densification et des microstructures finales entre une poudre broyée et une poudre non broyée est dressé. Enfin, l'influence de l'application d'une contrainte dynamique pendant la compaction au moyen d'un dispositif original est présentée / This work focuses on the microstructure evolution of a TiAl alloy during sintering by a process called Spark Plasma Sintering (SPS). The initial powders, elaborated by atomization, consist primarily of a metastable phase. The transformations of the return to equilibrium of the latter during heating are finely characterized using SEM, TEM and EBSD. These phase transformations are then used as a thermal indicator during the SPS densification to estimate the thermal and mechanical gradients. The densification mechanisms responsible for the neck formation and the origins of the microstructure heterogeneities of fully densified samples are discussed. A comparison between the densification mechanisms and the final microstructures of a milled powder and a no milled powder is showed. Finally, the effect of the application of a dynamic stress during the compaction using an original process is presented

Ultra high temperature ceramics (UHTC) are candidate materials for high temperature applications such as leading edges for hypersonic flight vehicles, thermal protection systems for spacecraft, and rocket nozzle throat inserts due to their extremely high melting points. Tantalum and Niobium Carbide (TaC and NbC), with melting points of 3950°C and 3600°C, respectively, have high resistivity to chemical attack, making them ideal candidates for the harsh environments UHTCs are to be used in. The major setbacks to the implementation of UHTC materials for these applications are the difficulty in consolidating to full density as well as their low fracture toughness. In this study, small amounts of sintering additive were used to enhance the densification and Graphene Nanoplatelets (GNP) were dispersed in the ceramic composites to enhance the fracture toughness. While the mechanisms of toughening of GNP addition to ceramics have been previously documented, this study focused on the anisotropy of the mechanisms. Spark plasma sintering was used to consolidate both bulk GNP pellets and near full relative density TaC-NbC ceramic composites with the addition of both sintering aid and GNP and resulted in an aligned GNP orientation perpendicular to the SPS pressing axis that allowed the anisotropy to be studied. In situ high load indentation was performed that allowed real time viewing of the deformation mechanisms for enhanced analysis. The total energy dissipation when indenting the bulk GNP pellet in the in-plane GNP direction was found to be 270% greater than in the out-of-plane orientation due to the resulting deformation mechanisms that occurred. In GNP reinforced TaC-NbC composites, the projected residual damaged area as a result of indentation was 89% greater when indenting on the surface of the sintered compact (out-of-plane GNP orientation) than when indenting in the orthogonal direction (in-plane GNP orientation) which is further evidence to the anisotropy of the GNP reinforcement.

published_or_final_version / Mechanical Engineering / Doctoral / Doctor of Philosophy

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Most recent developments in the production, properties and applications of borides and carbides are reviewed. The reactivity and sintering of finely-divided boron carbide with metal additives has been investigated. The additives (Fe, T i , Zr, V, Nb, Ta, Mo, W and Al) generally promote sintering of the boron carbide. Their effectiveness is reduced occasionally when there is some surface activation caused by the metals reacting vjith the boron carbide to form metal borides and carbides of different, crystal lattice type and molecular volume. The more metallic character of the bonding in the metal borides and carbides enhances surface and crystal lattice diffusion at the grain boundaries of the more covalent boron carbide. Iron is much more effective than the other metal addives tested in promoting sintering of the boron carbide at 1800 degree C since it forms the lowest-melting borides. It also enhances sintering during hot pressing of boron carbide at this temperature.

Thesis (M.Sc.(Engineering)--University of the Witwatersrand, Faculty of Engineering and the Built Environment, School of Chemical and Metallurgical Engineering, 2012,. / The objective of this research was to improve alumina (Al2O3) mechanical and electrical properties by reinforcement using multi-walled carbon nanotubes (MWCNTs) and titanium carbide (TiC). The objective of the study was achieved with interesting and challenging difficulties along the way. The MWCNTs were initially coated with boron nitride (hBN) in order to improve the Alumina-CNTs interface which was previously discovered to be weak and also to protect them from reacting with Al2O3 during sintering. The coating of CNTs with hBN was done using nitridation method. This method was unsuccessful since it was not possible to coat each CNT individually. Dispersing hBN coated CNTs proved to be impossible without pealing the off the hBN coating. The “flaking off “of the hBN coating from the CNTs revealed that the CNT-hBN interface was weak; therefore uncoated CNTs were used for this study. The starting powders (Al2O3, TiC and CNTs) were individually dispersed before they were mixed together. TiC and Al2O3 were dispersed using an ultrasonic probe which was done successfully. The CNTs were dispersed by an ultrasonic probe and then attritor milled with the use of polyvinylpyrolidone (PVP) as a dispersant. The dispersed Al2O3 and TiC (30 wt%) powders were mixed in a planetary ball mill. The composite powder was sieved and sintered using SPS with temperature and pressure programmed to be 1700˚C, 35MPa respectively. In making the Al2O3+CNT composite powder, the already dispersed Al2O3 and CNTs (1 wt%) were mixed in a planetary ball mill, after sieving the powder it was sintered using SPS at 1600˚C, 35MPa (programmed conditions). Lastly in making the Al2O3+CNT+TiC composite, the already dispersed TiC, CNTs and Al2O3 were all mixed in a planetary ball mill, after sieving it was sintered using SPS at 1650˚C, 35MPa (programmed conditions). For comparison of properties, dispersed monolithic Al2O3 was also sintered using SPS at 1600˚C, 35 MPa. The density results showed that the monolithic Al2O3 was 99.8% dense, , Al2O3+CNTs was 99.4%, Al2O3+TiC+CNTs was 99.2% and Al2O3+TiC sample was 99.0%. The mechanical properties of the samples were measured using the indentation method. The hardness and fracture toughness of the samples were; Al2O3= 3.3MPa√m (17 GPa), Al2O3+CNTs = 4.2MPa√m (18 GPa), Al2O3+TiC = 4.8 MPa√m (23 GPa) and Al2O3+TiC+CNT= 5.0 MPa√m (23 GPa). The electrical properties showed that incorporating CNTs and TiC into Al2O3 improved Al2O3 electrical conductivity. The measured electrical conductivity of the ceramic samples were; Al2O3 iii ≈ 0 Sm-1, Al2O3+CNTs= 30 S.m-1, Al2O3 +TiC + CNTs = 6855 S.m-1 and Al2O3+TiC = 9664 S.m-1. The CNTs improved Al2O3 mechanical properties slightly inhibiting grain growth by pinning the grain boundary movement and also by crack bridging. The Al2O3 electrical conductivity was increased by the CNTs network that was located along the alumina grain boundaries. The TiC improved Al2O3 mechanical properties slightly inhibiting grain growth and through crack deflection mechanism. The addition of TiC into Al2O3 increased the electrical conductivity by serving as a conducting continuous secondary phase. The results show that the CNT-hBN interface is weak. The addition of CNTs and TiC into monolithic Al2O3 slightly improved its mechanical and electrical properties but it density was slightly compromised. CNTs and TiC slightly improved monolithic alumina hardness by in inhibiting Al2O3 grain growth and the fracture toughness through crack deflection and crack bridging mechanisms. The CNTs network located at the Al2O3 grain boundaries not only aided in improving Al2O3 hardness but also served as transport medium for electrons hence increasing the Al2O3 electrical conductivity. Addition of TiC into Al2O3 increased its electrical conductivity by conducting electrons from one TiC grain to the adjacent grain. The large increase in electrical conductivity upon addition of TiC is due to the presence of a continuous TiC phase within Al203.